The present invention relates to a process for preparing compositions comprising oil soluble ingredients for use in the maintenance and/or promotion of health. In particular the invention relates to compositions for products for internal or external use by humans or animals such as beverages and capsules, processes for preparing such compositions and products containing them.
WO/94/06310 discloses an aqueous composition for the preparation of optically clear products for use in human and animal healthcare comprising 0.1 to 2.0% of an oil soluble ingredient as a 20-30% dispersion in a suitable oil or 0.1 to 5.0% w/v as the pure crystalline compound 2-20% of an emulsifier mixture having an HLB value of between 10 and 18 or where a blend of emulsifiers is employed, a calculated HLB value of between 10 and 18 and 0.1% of an antioxidant or a mixture of antioxidants.
In xe2x80x9cMicroemulsions Theory and Practicexe2x80x9d (Edited Leon M Prince chapter 3, Academic Press Inc, NY, 1977) it is stated that stable microemulsions result when an emulsifier is chosen that is chemically matched to the oil. Also in order to form satisfactory emulsions it can be helpful to use two kinds of emulsifier, a primary surfactant and a cosurfactant.
However, a problem encountered with existing compositions has been the stability of emulsions in the presence of certain carbohydrates (particularly syrups) especially those containing polymerised molecules. A particular problem is the formation of occlusion compounds or complexes on long term (several months) storage.
We have now found that a composition having enhanced bioavailability and stability in syrup can be obtained by using an emulsifier mixture comprising fatty acid residues which chemically matches the fatty acid residues of the oil soluble ingredient or a dispersion of the oil souluble ingredient and using specific ratios of oil or oil dispersion to emulsifier and specific ratios of primary to cosurfactant.
Accordingly, the present invention provides a process for preparing an aqueous composition for the preparation of optically clear products having enhanced stability in syrup and bioavailability for human or animal healthcare comprising
a) mixing 0.001-2.0% of an oil soluble ingredient or 0.1-2.0% w/w of an oil soluble ingredient as a 20-30% dispersion in a suitable oil with 2-10% of an emulsifier mixture having an HLB (hydrophilic lipophilic balance) value of between 10 and 18 and heating to between 25 and 150xc2x0 C. so as to yield a transparent mixture
b) combining the mixture with water while continuously stirring to provide a transparent composition
characterised in that the emulsifier mixture is a combination of a primary surfactant and a secondary or cosurfactant, wherein the fatty acid profile of the emulsifier mixture matches the fatty acid profile of the oil soluble ingredient or the dispersion of an oil soluble ingredient, the HLB of the primary surfactant is greater than the cosurfactant and the weight ratio of oil or oil dispersion to emulsifier is between 1:1 and 1:7 and the ratio of primary to cosurfactant is between 10:1 and 200:1.
Preferably the ratio of oil or oil dispersion to emulsifier is between 1:1 and 1:5. Preferably the ratio primary to cosurfactant is between 20:1 and 50:1, and is most suitably about 30:1.
Surprisingly, in addition to solving the problem of the formation of occlusion complexes, it has been found that by including a small amount of a cosurfactant allows less overall emulsifier is used. This is particularly valuable in the case of syrup containing beverages where reducing emulsifier content has cost and taste benefits and reduces the amounts of xe2x80x98syntheticxe2x80x99 components.
The present invention allows the formation of stable compositions in syrups which are typically up to 60 Brix, using very low amounts of emulsifier. This is particularly useful in the formulation of products especially energy drinks and capsules where excess amounts of emulsifiers along with carbohydrates can lead to the formation of occlusion products during long term (several months) storage.
An important advantage of the compositions of the present invention over known compositions is one of economy since it allows products with minimal amounts of emulsifiers to be developed. The compositions are particularly useful for incorporation of biologically active oils into aqueous preparations in a microdispersed form that facilitates uptake.
Preferably the mixture in a) is added to the water. Preferably one or more antioxidant(s) is first dispersed with the emulsifiers in a). Suitably the oil soluble ingredient is a biologically active oil by which we mean natural or synthetic oils which are or contain biologically active agents in particular prophylactic or therapeutic agents.
The composition of the present invention is able to yield a product with desirable properties, particularly high water solubility, using ingredients which have hitherto been found to be difficult to solubilise satisfactorily in this kind of product.
Preferably the biologically active oil is an oil of natural origin for example from the seeds or flowers of the Ribes. Boraginaceae, Labiataea, Onagraceae and Curcubitaceae species, oils of fungal origin, fish oils or other natural oils. Preferred oils include evening primrose oil, borage/starflower oil and blackcurrant seed oil. Preferably the oil soluble ingredient comprises a colouring ingredient.
Compositions containing xcex2 carotene as an oil soluble ingredient have been particularly successful. Particularly suitable sources of xcex2 carotene include both natural and synthetic xcex2 carotene as dispersions in oil (as available from various commercial sources including those mentioned herein).
Suitably the amount of oil is 0.001-2.0%, preferably 0.1-1.0% by weight expressed as the pure substance. Oils for use in the present invention can be extracted from natural sources by processes known in the art. The oils are commercially available, for example, from Sigma Chemical Co., Poole, Dorset. The compositions can contain more than one biologically active oil.
Other biologically active ingredients can be used in the composition according to the invention, in particular carotenoid pigments eg. xcex2 carotene to produce a useful combination of colour and nutritional biochemicals.
The biologically active oils may be mixed or dispersed with other suitable oils in particular, consumable oils for example, corn, peanut, safflower, olive and rapeseed oils as well as many essential oils particularly those used in beverages used to give flavours, such as citrus oils.
The emulsifiers may be any anionic, cationic, amphoteric or non-ionic emulsifier which are suitable for consumption by or application to the human or animal body. Preferably the emulsifiers are non-ionic emulsifiers having an HLB (hydrophilic/lipophilic balance) of 12-16 and most preferably has an HLB value of 15. Preferred mixtures include Tween 80 (polyoxyethylenesorbitan monooleate) and Span 80 (sorbitan monooleate) available from ICI Speciality Chemicals, Leatherhead, Surrey or from Sigma Chemical Company, Poole, Dorset.
Suitably the emulsifier mixture is a binary or tertiary blend of emulsifiers, for example blends of Tween 60 with a sucrose ester emulsifier (manufactured by Mitsubishi Kasei Food Corporation, Ichikawa Building, 13-3 Ginza 5-Chome, Chuo-ku, Tokyo 104, Japan) or blends of Tween 60 and sucrose ester and a polyglycerol ester of a fatty acid (available from Grindsted Products Limited., Northern Way, Bury St. Edmunds, Suffolk).
The amount of emulsifier mixture in the composition is selected as an amount which will vary depending upon which specific biologically active oil is used, its method of preparation, and how much is included. For example an oil-based dispersion containing 1% by weight of biologically active oil will generally require an emulsifier mixture in the range of 1-8-% w/w to achieve a clear dispersion and so as not to have significant adverse flavour effects in typical products when diluted.
Preferably the emulsifier mixture comprises a polysorbate, in particular polysorbate 60 in the case of consumable products as it has the advantage of having the least noticeable taste. Therefore, a particularly useful feature of the present invention is the ability to produce a flavourless composition.
The composition advantageously comprises in addition an antioxidant which can be for example, alpha-tocopherol, tocopheryl acetate , ascorbic acid, ascorbyl palmitate, butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) or a mixture of such antioxidants. Particularly preferred antioxidants are xcex1-tocopherol, tocopheryl acetate, ascorbyl palmitate and ascorbic acid.
Whilst the present invention is particularly useful in the production of optically clear products, the present invention can also be used to prepare opaque, cloudy products. A frequent problem with such products, particularly those products containing emulsified oils is that of xe2x80x98neck ringingxe2x80x99. The compositions prepared according to the present invention have been found not to exhibit this problem. It will be appreciated that the compositions of the present invention may be used for products in the pharmaceutical or veterinary field other than beverages, such as vitamin and cough syrups, throat sprays, lotions and mouthwashes, particularly where optical clarity is important.
Certain biologically active oils contain vitamins and provitamins such as vitamins A, D, E, carotenoid pigments and nutritionally important fatty acids.
In the compositions of the present invention the biologically active oils are believed to be finely dispersed in a micellar form or as microemulsions because they exhibit certain characteristics eg. transparency when viewed by transmitted light. Therefore a further advantage of the compositions according to the present invention is that the fine dispersion of these oils in aqueous preparations will help to promote their efficient uptake by body tissues when the composition is presented to the body. Whilst the small particle size of the particles of biologically active oils favour their uptake, the simultaneous presentation or ingestion of the oils with an emulsifier will also encourage efficient transfer of these substances across membranes.
The formulations according to the invention also have acid resistance. This is advantageous because prior to absorption from the intestinal tract, the preparation is able to survive the strongly acid conditions of the stomach.
In a further aspect of the invention there is provided a method of administration of an oil-soluble material to human or animal body by treating said body with a composition according to the invention. Preferably the composition is administered orally, for example in the form of a liquid composition.
The composition obtained according to the present invention is an aqueous dispersion which is capable of dissolution in water-based products to yield optically clear finished products. It will be appreciated that further ingredients may optionally be included in the composition of the present invention or to the final food product, for example sweeteners, preservatives (eg. sulphur dioxide, benzoic acid and sorbic acid), proteins, fats, vitamins, minerals and other materials employed in the preparation of food and drink products. Optionally the compositions also contain antioxidant cofactors such as zinc, selenium and manganese which are needed for the body""s naturally occurring antioxidant enzymes. Preferably the final product is flavoured; this can be achieved by the addition of naturally flavoured foods such as fruit juices and concentrates, extracts and compounds or flavouring additives. Preferably further nutritive ingredients are added to the final drink such as other vitamins and minerals as described in xe2x80x9cThe Food Labelling Regulations 1984xe2x80x9d Statutory Instrument No. 1305 (1984) H.M.S.O., London.
Suitably processing aids can be incorporated. Such aids may include ingredients which influence pH, redox potential, enzyme activity, hydrogen bonding and/or other aspects. Processing aids are for example sulphur dioxide, other antioxidants, metal salts, acids (eg. phosphoric and citric acid), alkalis, surfactants such as lecithin and starch plasticisers eg. calcium chloride. Preferred processing aids for inclusion are anti-foaming agents eg. silicones.
Ingredients subject to a loss of nutritional value are added at a late stage of the process. Optionally the product can be produced in light or oxygen excluding containers after preparation to increase protection of materials sensitive to light or oxygen induced degradation. Optionally the product can be carbonated.
The use of these high temperatures incurs the risk of degradation of the oil unless suitable precautions are taken. For example it is desirable to exclude oxygen by heating the mixture in an atmosphere of nitrogen. In a further aspect of the present invention additional water is added to the composition to yield an aqueous intermediate product which is suitable for use in a suitable water-based product.
In a further aspect of the invention there is provided the use of carotene microemulsions to deliver high bioavailability carotenes to the blood and to tissues for use in medicine. The invention is illustrated by the following Examples.